高效液相色谱法测定动物组织中氟苯达唑、噻苯达唑及代谢物残留量的研究
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- 英文论文题名：Simultaneous Determination of Flubendazole and Thiabendazole and Their Metabolites Residues in Animal Tissues by High Performance Liquid Chromatography
- 论文作者：李丹 ; 张玉洁 ; 王鹤佳 ; 李倩 ; 李莉 ; 薛毅 ; 仲锋
- 英文论文作者：LI Dan ; ZHANG Yu-jie ; WANG He-jia ; Li Qian ; Li Li ; XUE Yi ; ZHONG Feng ; China Institute of Verterinary Drug Control ; The Ningxia Hui Autonomous Region veterinary drug feed monitoring Institute ; Chinese Center of Animal Disease Control
- 年：2016
- 作者机构：中国兽医药品监察所;宁夏回族自治区兽药饲料监察所;中国动物疫病预防控制中心;
- 论文关键词：高效液相色谱法 ; 氟苯达唑 ; 噻苯达唑 ; 代谢物 ; 残留 ; 猪组织 ; 牛组织
- 英文论文关键词：HPLC ; flubendazole ; thiabendazole ; metabolites ; residue ; pig tissues ; cattle tissues
- 会议召开时间：2016-09-18
- 会议录名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会论文集
- 语种：中文
- 分类号：S859.84;O657.72
- 学会代码：ZGXJ
- 会议名称：中国畜牧兽医学会动物药品学分会第五届全国会员代表大会暨2016年学术年会
- 会议地点：中国四川成都
- 主办单位：中国畜牧兽医学会动物药品学分会
- 学会名称：中国畜牧兽医学会
- 页数：7
- 文件大小：424k
- 原文格式：O
- 会议级别：全国
摘要
建立一种可同时检测猪、牛组织(肌肉、肝脏、肾脏、脂肪、牛奶)中氟苯达唑及代谢物2-氨基氟苯达唑、噻苯达唑及代谢物5-羟基噻苯达唑药物残留的高效液相色谱—紫外检测法。猪、牛组织样品经乙腈提取,加入Na_2SO_4盐析去杂质,异辛烷去脂肪,MCX柱净化。以0.02 mol/L乙酸铵溶液和乙腈溶液为流动相,梯度洗脱,检测波长306 nm。结果表明氟苯达唑及代谢物2-氨基氟苯达唑、噻苯达唑及代谢物5-羟基噻苯达唑在0.01-2.0μg/mL呈良好的线性关系,r均大于0.99。猪、牛组织中方法的最低定量限分别为5μg/kg、20μg/kg。猪、牛组织中氟苯达唑及代谢物2-氨基氟苯达唑、噻苯达唑及代谢物5-羟基噻苯达唑分别在5-200μg/kg、20-200μg/kg的浓度添加水平上,其回收率范围在60~100%之间,批内相对标准偏差小于15%、批间相对标准偏差小于20%。
A high performance liquid chromatography(HPLC) method has been developed for the simultaneous determination of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites of 2-aminoflubendazole(2-NH_2-FLUB),5-hydroxythiabendazole(5-OH-TBZ)in pig and cattle tissues(muscle,liver,kidney,fat,milk).Sample was extracted by acetonitrile and was spiked Na_2SO_4,then degreased by isooctane and dissolved with 30%acidified alcohol after evaporation,the solution was purified with MCX column.The separation of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites was performed with the gradient elutinon solvent of 0.02 mol/L ammonium acetate and acetonitrile,and detection wavelengths was 306 nm.A good linearity of the calibration curve was obtained with the range of 0.01-2.0 μg/mL(R~2>0.99)t and the limit of quantification for pig and cattle was 5 μg/kg and 20 μg/kg,respectively.The average recoveries of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites of 2-arninoflubendazole(2-NH_2-FLUB),5-hydroxythiabendazole(5-OH-TBZ) from spiked pig and cattle tissues between 5~200 μg/kg and 20~200 μg/kg both ranged from 60-100%(n=5).Intra-day batch variation coefficients were less than 15%and inter-day batch variation coefficients were both less than 20%.
A high performance liquid chromatography(HPLC) method has been developed for the simultaneous determination of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites of 2-aminoflubendazole(2-NH_2-FLUB),5-hydroxythiabendazole(5-OH-TBZ)in pig and cattle tissues(muscle,liver,kidney,fat,milk).Sample was extracted by acetonitrile and was spiked Na_2SO_4,then degreased by isooctane and dissolved with 30%acidified alcohol after evaporation,the solution was purified with MCX column.The separation of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites was performed with the gradient elutinon solvent of 0.02 mol/L ammonium acetate and acetonitrile,and detection wavelengths was 306 nm.A good linearity of the calibration curve was obtained with the range of 0.01-2.0 μg/mL(R~2>0.99)t and the limit of quantification for pig and cattle was 5 μg/kg and 20 μg/kg,respectively.The average recoveries of flubendazole(FLUB),thiabendazole(TBZ) and their metabolites of 2-arninoflubendazole(2-NH_2-FLUB),5-hydroxythiabendazole(5-OH-TBZ) from spiked pig and cattle tissues between 5~200 μg/kg and 20~200 μg/kg both ranged from 60-100%(n=5).Intra-day batch variation coefficients were less than 15%and inter-day batch variation coefficients were both less than 20%.
引文
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[10]李丹,张玉洁,汪霞,等.高效液相色谱法检测羊鸡组织中氟苯达唑、噻苯达唑及其代谢物残留量的研究[J].中国兽药杂志,2011,45(6):26-30.
[2]陈杖榴.兽医药理学(第二版)[M].北京:中国农业出版社,2002:282
[3]Lipka E,Charton J,Vaccher C.Development of HPLC/fluorescence detection method for chiral resolution of dansylated benzimidazoles derivatives[J].Biomedical Chromatography,2014,28(1):4-9.
[4]Yanawath S,Rodjana B.Alternative Green Preconcentration Approach Based on Ultrasound-Assisted Surfactant-Enhanced Emulsification Microextraction and HPLC for Determination of Benzimidazole Anthelmintics in Milk Formulae Tittaya Boontongto[J].Chromatographia,2014,77(21/22):1557-1562.
[5]Takao C,Kazuhiko N,Yuzi H.Rapid Determination of Residues of Five Kinds of Veterinary Drugs in Livestock Products by HPLC[J].食品衛生学雜誌,2000,41(5):326-329.
[6]Takeba K,Fujinuma K,Sakamoto M,et al.Determination of benzimidazole a nthelmintics in livestock foods by HPLC[J].食品衛生学雜誌,2003,44(5):246-252.
[7]Moreno.L,Alvarez.L,Lanusse.C,et al.Multiresidue HPLC method to measure benzimidazole anthelmintics in plasma and egg from laying hens.Evaluation of albendazole metabolites residue profiles[J].Food Chemistry,2011,126(2):793-800.
[8]Liu H,Jiang C,Hui Y,et al.SPE-LC multi-residue analysis of mebendazole and its metabolites in grass carp and shrimp[J].Chromatographia,2010,72(11/12).1083-1088.
[9]李俊锁,邱月明,王超.兽药残留分析[M].上海:上海科学技术出版社,2002:40.
[10]李丹,张玉洁,汪霞,等.高效液相色谱法检测羊鸡组织中氟苯达唑、噻苯达唑及其代谢物残留量的研究[J].中国兽药杂志,2011,45(6):26-30.